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目的:建立能同时分离分析大鼠尿样中延胡索乙素(THP)及其代谢产物的HPLC/DAD方法。方法:尿样经Oasis HLBC18固相萃取小柱提取,采用HPLC/DAD法检测,色谱柱:Ultimate XB-C18(4.6mm×200mm,5μm);流动相:A相为0.1%醋酸水溶液(三乙胺调节pH5.5),B相为乙腈,梯度洗脱;流速为1.0mL·min-1;检测波长230nm;大鼠给药THP后,收集其尿样分析。结果:THP在0.10～50.0μg·mL-1的范围内有良好的线性关系(r=0.9999),最低定量限为0.10μg·mL-1,平均方法回收率为99.5%,提取回收率为73.6%;日内和日间RSD小于9%。结论:所建立的方法准确可靠,可用于THP尿样浓度测定及其排泄动力学研究。
OBJECTIVE: To establish an HPLC / DAD method for the simultaneous separation and analysis of tetrahydropalmatine (THP) and its metabolites in rat urine samples. Methods: Urine samples were extracted with Oasis HLBC18 solid phase extraction cartridge and detected by HPLC / DAD. The mobile phase consisted of 0.1% acetic acid aqueous solution (A) Amine was adjusted to pH 5.5), acetonitrile (B phase) and gradient elution. The flow rate was 1.0 mL · min-1 and the detection wavelength was set at 230 nm. Urine samples were collected from rats after administration of THP. Results: The linear range of THP was 0.10 ~ 50.0μg · mL-1 (r = 0.9999), the lowest limit of quantification was 0.10μg · mL-1, the average recovery was 99.5% and the recovery was 73.6 %; Day and day RSD less than 9%. Conclusion: The established method is accurate and reliable and can be used for the determination of urinary concentration of THP and its excretion kinetics.